CN113695591A - 316L stainless steel indirect 3D forming method based on fused deposition - Google Patents

316L stainless steel indirect 3D forming method based on fused deposition Download PDF

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CN113695591A
CN113695591A CN202110921611.XA CN202110921611A CN113695591A CN 113695591 A CN113695591 A CN 113695591A CN 202110921611 A CN202110921611 A CN 202110921611A CN 113695591 A CN113695591 A CN 113695591A
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printing
temperature
stainless steel
blank
parameters
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CN113695591B (en
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袁艳萍
相世博
陈继民
张成宇
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Beijing University of Technology
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Beijing University of Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/10—Formation of a green body
    • B22F10/16—Formation of a green body by embedding the binder within the powder bed
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/60—Treatment of workpieces or articles after build-up
    • B22F10/62—Treatment of workpieces or articles after build-up by chemical means
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/60—Treatment of workpieces or articles after build-up
    • B22F10/64—Treatment of workpieces or articles after build-up by thermal means
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/1017—Multiple heating or additional steps
    • B22F3/1021—Removal of binder or filler
    • B22F3/1025—Removal of binder or filler not by heating only
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
    • B33Y40/20—Post-treatment, e.g. curing, coating or polishing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Civil Engineering (AREA)
  • Composite Materials (AREA)
  • Structural Engineering (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention relates to the technical field of metal 3D printing, in particular to a 316L stainless steel indirect 3D forming method based on fused deposition. The high-density 316L stainless steel part is prepared by taking the composite wire of 316L stainless steel powder and a high-molecular binder as raw materials and combining two technologies of fused deposition 3D printing and heat treatment. The invention provides a low-cost, economical and large-scale metal 3D printing indirect manufacturing method, which has important significance for realizing wide application of metal 3D printing and promoting the development of the manufacturing industry in China.

Description

316L stainless steel indirect 3D forming method based on fused deposition
Technical Field
The invention relates to the technical field of metal 3D printing, in particular to a method for indirectly forming 316L stainless steel based on Fused Deposition Modeling (FDM) (fused Deposition modeling)3D printing technology.
Background
In recent years, 3D printing technology has become an indispensable technology in manufacturing industry due to the advantages that conventional manufacturing technologies, such as parts with arbitrary shapes can be processed, personalized customization and integral molding, do not have. The metal materials such as iron-based alloy, titanium alloy, aluminum alloy and the like are widely applied in 3D printing and play an important role in the fields of industrial manufacturing, biomedical treatment, aerospace and the like. At present, metal materials are generally processed by selective laser melting, selective electron beam melting, laser near-net shaping and other technologies, the technologies all adopt high-energy-density laser beams or electron beams as heat sources for direct 3D printing and shaping, and the prepared metal parts can obtain good performance. However, the direct metal 3D printing equipment is expensive, the use cost is high, and the occupied area of the whole machine is large, which all limit the further development of the metal 3D printing technology, so that the metal 3D printing technology is not applied in a large scale from birth to the present. Therefore, the cost of metal 3D printing is reduced, and the method has important significance for realizing wide application of metal 3D printing and promoting the development of the manufacturing industry in China.
Disclosure of Invention
The invention aims to provide a low-cost, economical and large-scale applicable metal 3D printing indirect forming method, which takes a composite wire of 316L stainless steel powder and a high-molecular binder as a raw material and combines two technologies of fused deposition 3D printing and heat treatment to prepare a high-density 316L stainless steel part.
According to the preparation requirement, the invention adopts the following materials and equipment: 316L stainless steel powder and polymer binder, wherein the grain diameter of the 316L stainless steel powder is less than or equal to 20 μm, and the average diameter of the wire is 1.76 mm; 99.5% cyclohexane solution; an FDM 3D printer; a constant-temperature water bath kettle; a vacuum tube furnace.
The invention is realized by the following technical steps:
first, the creation and processing of a three-dimensional model.
And creating a three-dimensional model of the part by using three-dimensional modeling software according to actual requirements, carrying out layering processing on the three-dimensional model of the part by using slicing software, and setting printing parameters such as printing temperature, printing speed, filling mode, layering thickness, extrusion multiplying power, filling rate and the like.
And secondly, 3D printing of the part blank.
Firstly, importing a Gcode file carrying printing parameters into an FDM 3D printer; then, preheating a printing nozzle and a printing substrate of the FDM 3D printer; then, loading a printing material after preheating is finished; and finally, manufacturing a part blank according to the set printing parameters and the planned printing path.
And thirdly, degreasing the part blank by using a solvent.
And soaking the printed part blank in a cyclohexane solution with the mass percentage concentration of 99.5% in a constant-temperature water bath kettle to degrade a thermoplastic elastomer in the high-molecular binder and form a microscopic pore channel in the blank, so that the subsequent heat treatment effect is improved, and the forming quality of the part is improved.
And fourthly, cleaning and drying the part blank.
And (3) placing the part blank degreased by the solvent into a beaker filled with an acetone solution for ultrasonic cleaning for 5min, and then placing the part blank into a beaker filled with alcohol for ultrasonic cleaning for 3min to remove residual organic pollutants on the surface of the blank. And putting the cleaned blank into a drying box for full drying.
And fifthly, performing heat treatment on the part blank.
The vacuum tube furnace is used for carrying out heat treatment on the part blank, and the process is completed in two stages. In the first stage, degreasing is carried out at the temperature of less than 800 ℃ so as to remove residual high molecular polymer in the blank. And the second stage is sintering at temperature higher than 1300 deg.c to produce compact metal parts.
And sixthly, testing the performance of the stainless steel part.
And observing the surface appearance of the part through an optical microscope, a scanning electron microscope and a laser confocal microscope, and analyzing the forming quality of the part. And measuring the density of the part by an Archimedes drainage method. The mechanical properties of the parts were measured by means of a microhardness tester and a universal tester.
The invention has the beneficial effects that:
(1) the compact 316L stainless steel part is prepared by combining the fused deposition 3D printing technology and the heat treatment technology, and has the advantages of low manufacturing cost, high forming precision, convenience in operation and the like;
(2) the invention researches the fused deposition forming process parameters of the composite wire consisting of 316L stainless steel powder and a high polymer binder, and researches the degreasing sintering process parameters of a blank body;
(3) the invention indirectly prepares the 316L stainless steel part based on the fused deposition forming technology, obtains good performance and can better meet the practical application;
(4) according to the invention, the metal parts are indirectly printed in a 3D manner in a low-cost and economical manner, so that the cost of metal 3D printing is greatly reduced, and the method has an important significance for large-scale application of metal 3D printing.
Drawings
Fig. 1 is a schematic flow chart of a fused deposition-based 316L stainless steel indirect 3D forming method.
Fig. 2 is a physical diagram of sample blanks made at different printing temperatures in example 1, where (a) the printing temperature was 230 ℃, (b) the printing temperature was 250 ℃, and (c) the printing temperature was 270 ℃.
FIG. 3 is SEM images of the degreasing effect of the solvent at different temperatures in example 1, wherein (a) the temperature is 45 deg.C, (b) the temperature is 55 deg.C, and (c) the temperature is 65 deg.C.
FIG. 4 is an SEM image of the thermal degreasing effect at different temperatures in example 1, wherein (a) the temperature is 500 deg.C, (b) the temperature is 600 deg.C, (c) the temperature is 700 deg.C, and (d) the temperature is 800 deg.C.
Fig. 5 is a surface topography map of a 316L stainless steel sample prepared indirectly based on fused deposition, wherein (a) is an optical microscope photograph and (b) is a scanning electron microscope photograph.
Detailed Description
The technical solution of the present invention is further described in detail with reference to the accompanying drawings.
Example 1:
firstly, designing a three-dimensional model of a part by using Solidworks software, carrying out layering processing on the three-dimensional model by using Simplify3D software, and simultaneously setting printing parameters such as printing temperature, printing speed, filling mode, layering thickness, extrusion multiplying power, filling rate and the like. Preferably, the printing temperature must be > 220 ℃. Preferably, the printing speed is selected to be 20mm/s, and the printing speed is not recommended to exceed the value for ensuring the printing forming quality. The mechanical properties of parts manufactured by three filling modes, namely Recilinear, Triangular and Honeycnmb, are simulated by using ANSYS workbench software, and Triangular is used as a preferred filling mode according to the simulation result. Preferably, the layer thickness is set to 0.2mm, improving printing efficiency while ensuring forming quality. Preferably, the extrusion magnification is set to 110% in order to improve the compactness of the formed body. Preferably, the filling rate is set to 100%.
Secondly, firstly, importing a Gcode file carrying printing parameters into an FDM 3D printer; then preheating a printing nozzle and a printing substrate of the FDM 3D printer, and preferably setting the temperature of the printing substrate to be 40 ℃; then, loading a printing material after preheating is finished, stopping loading when a molten wire is observed to be extruded from a nozzle of the FDM 3D printer, and cleaning the extruded wire by using a scraper; and finally, printing the part blank according to the set printing parameters and the planned printing path.
Referring to fig. 2, the temperature at which the wire used in the present invention is melted is 220 ℃, and three printing temperatures of 230 ℃, 250 ℃ and 270 ℃ are set above the temperature to perform a control experiment, and preferably, it is determined that the forming quality of the blank is good when the printing temperature is 250 ℃.
And thirdly, carrying out chemical solvent degreasing on the printed part blank by adopting a 99.5% cyclohexane solution in a constant-temperature water bath kettle so as to degrade a thermoplastic elastomer in the high-molecular binder and form a microscopic pore channel in the blank, so that the subsequent heat treatment effect is improved, and the forming quality of the part is improved. As shown in fig. 3, chemical solvent degreasing is performed at three temperature groups of 45 ℃, 55 ℃ and 65 ℃ respectively, and micro-pores are formed in the sample at 55 ℃ and uniformly distributed, so that a good solvent degreasing effect is obtained, and therefore 55 ℃ is taken as a preferred solvent degreasing temperature. Preferably, the degreasing time by the chemical solvent is 24 h.
And fourthly, placing the part blank degreased by the solvent into a beaker filled with an acetone solution for ultrasonic cleaning for 5min, and then placing the part blank into a beaker filled with alcohol for ultrasonic cleaning for 3min, so as to fully remove the residual organic pollutants on the surface of the blank. And putting the cleaned blank into a drying box for full drying.
And fifthly, carrying out heat treatment on the part blank, namely carrying out degreasing and sintering treatment at high temperature to degrade residual high molecular polymers in the blank and sinter a compact metal part, wherein in order to avoid oxidation reaction of 316L stainless steel materials at high temperature, the heat treatment of a vacuum tube furnace is taken as a preferred scheme. And determining a key temperature node of heat treatment according to the TG-DSC test result of the printing sample blank, wherein the temperature of the high molecular polymer when the high molecular polymer starts to degrade is 340 ℃, and the temperature of the polymer when the polymer is completely degraded is 480 ℃, so that the temperature of thermal degreasing is necessarily higher than 480 ℃. When the blank is subjected to thermal degreasing, the blank needs to be kept at the highest thermal degreasing temperature for a certain time, so that the sample piece is sufficiently degreased and primary mechanical stability is realized. As shown in fig. 4, four sets of thermal degreasing temperatures of 500 ℃, 600 ℃, 700 ℃ and 800 ℃ are respectively set, sintering necks appear in all stainless steel particles in the sample at the temperature of 800 ℃, the stainless steel particles are filled by the sintering necks, and the mechanical property of the sample tends to be stable, so that 800 ℃ is taken as the optimal maximum temperature for thermal degreasing. In order to form the sample after the thermal degreasing into a dense metal part, the sample needs to be sintered at a high temperature after the thermal degreasing, and preferably, the sintering temperature is set to 1350 ℃.
Preferably, the heat treatment parameters of the present invention are: setting the heating rate below 300 ℃ to be 5 ℃/min; setting the heating rate of 300-800 ℃ to 1 ℃/min, and keeping the temperature at 800 ℃ for 1.5 h; heating from 800 ℃ to 1350 ℃ at the heating rate of 5 ℃/min, and preserving the heat for 2 hours at the highest sintering temperature; in the cooling stage, the temperature is reduced from 1350 ℃ to 500 ℃ by adopting a program temperature control (5 ℃/min), and the temperature is naturally reduced below 500 ℃.
And sixthly, observing the surface molding quality of the prepared metal sample through an optical microscope and a scanning electron microscope, wherein as shown in figure 5, the stainless steel part indirectly printed by 3D based on the fused deposition technology has no obvious air holes and crack defects, and obtains good surface appearance. The surface roughness of the sample piece measured by a confocal laser microscope was 3.74 μm, indicating that the surface of the sample piece was smooth. The density of the sample piece measured by an Archimedes drainage method reaches 94.23%. The microhardness value of a sample piece measured by using a microhardness tester is 131.36HV, and the tensile strength of the sample piece measured by using a universal testing machine is 343MPa, which shows that the metal sample piece prepared by the invention achieves good mechanical properties.
The above is a preferred embodiment of the present invention, and from the above, those skilled in the art can make various modifications and improvements on the basis of the above description, and any changes should fall within the protection scope of the claims of the present invention without departing from the technical idea of the present invention.

Claims (1)

1. A316L stainless steel indirect 3D forming method based on fused deposition is characterized by comprising the following steps:
1) creating a three-dimensional model of the part using three-dimensional modeling software;
2) layering a three-dimensional model of a part by using slicing software, and setting printing parameters, wherein the specific parameters are that the printing temperature is 250 ℃, the printing speed is 20mm/s, the filling mode is Triangular, the layering thickness is 0.2mm, the extrusion rate is 110%, and the filling rate is 100%;
3) importing a Gcode file carrying printing parameters into an FDM 3D printer, preheating a printing nozzle and a printing substrate of the FDM 3D printer, loading printing materials after preheating is finished, and preparing a part blank according to the set printing parameters and a planned printing path;
4) carrying out chemical solvent degreasing on the printed part blank for 24 hours by adopting a cyclohexane solution with the mass percentage concentration of 99.5% in a constant-temperature water bath kettle at the temperature of 55 ℃;
5) putting the part blank degreased by the solvent into a beaker filled with an acetone solution, carrying out ultrasonic cleaning for 5min, then putting the part blank into a beaker filled with alcohol, carrying out ultrasonic cleaning for 3min, and putting the cleaned blank into a drying oven for full drying;
6) degreasing and sintering the part blank in a vacuum tube furnace to prepare the metal part, wherein the specific heat treatment parameters are as follows: setting the heating rate below 300 ℃ to be 5 ℃/min; setting the heating rate of 300-800 ℃ to 1 ℃/min, and keeping the temperature at 800 ℃ for 1.5 h; heating from 800 ℃ to 1350 ℃ at the heating rate of 5 ℃/min, and preserving the heat for 2 hours at the highest sintering temperature; in the cooling stage, the temperature is reduced from 1350 ℃ to 500 ℃ by adopting a program temperature control mode of 5 ℃/min, and the temperature is naturally cooled below 500 ℃.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106822994A (en) * 2016-12-30 2017-06-13 浙江工业大学 A kind of stainless steel is implanted into composite material and its preparation and application
CN109095917A (en) * 2018-09-10 2018-12-28 北京工业大学 A kind of preparation method of the bioactivity, porous hydroxyapatite/Ti acid barium composite ceramics based on 3D printing
JP2019001008A (en) * 2017-06-12 2019-01-10 ボッシュ株式会社 Method of producing composite material molded article of cellulose fiber resin
CN109665819A (en) * 2018-12-10 2019-04-23 北京工业大学 A kind of preparation method of the porous minimal surface structure aluminium oxide ceramics based on 3D printing
CN109808035A (en) * 2019-01-21 2019-05-28 北京工业大学 A kind of compound porous bioceramic scaffold production method of hydroxyapatite/silica based on 3D printing
CN111940739A (en) * 2020-07-01 2020-11-17 中国第一汽车股份有限公司 Polymer composite stainless steel 3D printing material, preparation method and part preparation method

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106822994A (en) * 2016-12-30 2017-06-13 浙江工业大学 A kind of stainless steel is implanted into composite material and its preparation and application
JP2019001008A (en) * 2017-06-12 2019-01-10 ボッシュ株式会社 Method of producing composite material molded article of cellulose fiber resin
CN109095917A (en) * 2018-09-10 2018-12-28 北京工业大学 A kind of preparation method of the bioactivity, porous hydroxyapatite/Ti acid barium composite ceramics based on 3D printing
CN109665819A (en) * 2018-12-10 2019-04-23 北京工业大学 A kind of preparation method of the porous minimal surface structure aluminium oxide ceramics based on 3D printing
CN109808035A (en) * 2019-01-21 2019-05-28 北京工业大学 A kind of compound porous bioceramic scaffold production method of hydroxyapatite/silica based on 3D printing
CN111940739A (en) * 2020-07-01 2020-11-17 中国第一汽车股份有限公司 Polymer composite stainless steel 3D printing material, preparation method and part preparation method

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